Focusing on ammonium hydrogen fluoride surface treatment of aluminum enterprise wastewater which contained high-level NH3-N and fluoride ions, to pre-treat ammonium bifluoride wastewater to the concentration that has been confirmed in advance, flotation + chemical precipitation of magnesium ammonium phosphate(MAP) was used. Then the waste water was further treated in the Oxidative wastewater pool, so that it can reach the emission standard. After verification with experiments, this is not only technically feasible but also economically reasonable for removal of ammonium bifluoride wastewater.